Bhatt Mithun, Alok Anshu, Kulkarni Bhushan B
Mehsana Urban Institute of Sciences, Faculty of Science, Ganpat University, Mehsana 384012, India.
Department of Biotechnology, UIET, Panjab University, Chandigarh 160014, India.
BioTech (Basel). 2022 Jun 3;11(2):19. doi: 10.3390/biotech11020019.
Post-translational modifications ("PTMs") in monoclonal antibodies (mAbs) contribute to charge variant distribution, which will affect biological efficacy and safety. For the characterization of mAbs, charge variants are used as a critical quality attributes for product quality, stability consistency and effectiveness. Charge variants in mAbs are characterized by a time-consuming and a multistep process starting from cation/anion exchange chromatography, acidic/basic fractions collection and subsequent reverse phase (RP) liquid chromatography, coupled with mass spectrometry (MS) analysis. Hence, an alternative characterization approach that would be highly selective for ion exchange chromatography-based charge variant analysis, which is compatible with on-line MS detection, is needed in the biopharma industry. Against this backdrop, multiple studies are being conducted to develop a simple straight on-line charge variant analysis method. In this regard, we apply the current study, which aims to develop a charge variant analytical method, based on volatile buffers with low ionic strength that can be used for on-line MS detection of charge variants of mAbs. This would enable the detection on "PTMs" using low ionic strength mobile phase compatible with MS. Hence, fruitful data can be obtained with a single chromatography run without any test sample preparation, eliminating the need for multiple steps of analysis, time-consuming process and multiple sample preparation steps. Thus, Charge Variant Analysis-MS technique will allow the characterization of charge-related PTMs on the intact protein stage. In this regard, this study is about development of a method having combination of chromatography and volatile mobile phase for mass spectrometry detection of mAbs being analyzed in native form. The method is qualified considering pharmacopeia guidelines because the ultimate aim is to transfer this method for Quality Control (QC) release testing of a monoclonal antibody, which is critical for batch release and the regulatory point of view. Acidic and basic variants have been separated with high resolution peak profile. Furthermore, there was no matrix interference and good separation selectivity in terms of specificity was obtained using this method. The experimental data suggested for the linearity of the method are 2.4 mg/mL to 3.6 mg/mL with % RSD below 2.0%. Additionally, Limit of Quantitation is found to be 0.15 mg/mL, which is 5% of loading amount. Consistently, the data show that the method is precise under the same operating conditions with a short time interval. Overall a simple, accurate, robust and precise pH gradient cation exchange chromatography method was developed and qualified for the characterization of a therapeutic native mAb. Additionally, this method can be used to claim a biosimilar product profile of an in-house product compare to an innovator.
单克隆抗体(mAb)中的翻译后修饰(“PTMs”)会影响电荷变体分布,进而影响生物疗效和安全性。对于mAb的表征,电荷变体被用作产品质量、稳定性一致性和有效性的关键质量属性。mAb中的电荷变体通过一个耗时且多步骤的过程来表征,该过程从阳离子/阴离子交换色谱、酸性/碱性馏分收集以及随后的反相(RP)液相色谱开始,并结合质谱(MS)分析。因此,生物制药行业需要一种对基于离子交换色谱的电荷变体分析具有高选择性且与在线MS检测兼容的替代表征方法。在此背景下,正在进行多项研究以开发一种简单直接的在线电荷变体分析方法。在这方面,我们开展了当前这项研究,旨在开发一种基于低离子强度挥发性缓冲液的电荷变体分析方法,该方法可用于mAb电荷变体的在线MS检测。这将能够使用与MS兼容的低离子强度流动相来检测“PTMs”。因此,无需任何测试样品制备,通过一次色谱运行就能获得丰富的数据,无需多步分析、耗时的过程和多样的样品制备步骤。这样,电荷变体分析 - MS技术将能够在完整蛋白质阶段对与电荷相关的PTMs进行表征。在这方面,本研究是关于开发一种结合色谱和挥发性流动相的方法,用于以天然形式分析的mAb的质谱检测。考虑到药典指南,该方法是合格的,因为最终目标是将此方法用于单克隆抗体的质量控制(QC)放行检测,这对批次放行和监管角度而言至关重要。酸性和碱性变体已通过高分辨率峰形分离。此外,使用该方法在特异性方面没有基质干扰且具有良好的分离选择性。该方法的实验数据表明,线性范围为2.4 mg/mL至3.6 mg/mL,相对标准偏差(%RSD)低于2.0%。此外,定量限为0.15 mg/mL,即进样量的5%。一致地,数据表明该方法在相同操作条件下且时间间隔较短时是精确的。总体而言,开发了一种简单、准确、稳健且精确的pH梯度阳离子交换色谱方法,并对一种治疗性天然mAb的表征进行了验证。此外,该方法可用于宣称内部产品与创新产品相比的生物类似药产品概况。